CN106099064B - Preparation method of SnS2/CNTs composite nano material and application of composite nano material as negative electrode material of sodium-ion battery - Google Patents
Preparation method of SnS2/CNTs composite nano material and application of composite nano material as negative electrode material of sodium-ion battery Download PDFInfo
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention belongs to the technical field of novel secondary battery cathode materials and preparation thereof, and particularly relates to a preparation method of a SnS2/CNTs composite nano material and application of the SnS2/CNTs composite nano material as a sodium ion battery cathode material. Firstly, adding carbon nano tubes into ultrapure water and carrying out ultrasonic treatment; then adding SnCl4 & 5H2O solution and thiourea; then carrying out hydrothermal reaction to obtain the SnS2/CNTs composite nano material. When the composite material is used as a negative electrode material of a sodium ion battery, good conductivity and reversible capacity are shown, and the SnS2/CNTs has good application prospect as the negative electrode material of the sodium ion battery.
Description
Technical Field
the invention belongs to the technical field of novel secondary battery cathode materials and preparation thereof, and particularly relates to a preparation method of a SnS2/CNTs composite nano material and application of the SnS2/CNTs composite nano material as a sodium ion battery cathode material.
Background
sodium ion batteries, as a class of excellent energy storage devices, have been considered as an ideal substitute for lithium ion batteries due to their characteristics of abundant sources, simple preparation process, no pollution, certain excellent electrochemical properties, and the like. Similar to lithium ion batteries, sodium ion batteries are mainly composed of three parts, namely positive electrode materials, negative electrode materials and electrolyte, and the working principle of the sodium ion battery is realized by continuously extracting and embedding sodium ions between the positive electrode materials and the negative electrode materials.
Compared with lithium ions, the radius of sodium ions is much larger, so that the conventional lithium ion battery negative electrode material cannot be directly used as the sodium ion battery negative electrode material, and it is very important to find a negative electrode material suitable for the operation of the sodium ion battery.
The metal-based material is an ideal sodium ion battery cathode material due to the higher theoretical capacity of the metal-based material, and metal alloys, metal oxides and metal sulfides are common in the metal-based material. The SnS2 has CdI2 type crystal structure, which is a sandwich structure composed of two closely arranged S atoms and Sn cation sandwiches, and the layers are combined with weak van der Waals force. The SnS2 has good electrochemical performance as a sodium ion battery cathode material, and the theoretical capacity of the tin-based material can reach 847mAh/g based on the theoretical chemical calculation of Na15Sn4, so that the Sn-based material is a sodium ion battery cathode material with great potential.
however, during the cyclic de-intercalation process of sodium ions, the single SnS2 generates large volume change (about 420%) and low conductivity of the single SnS2, which limits the application of the single SnS2 as the negative electrode material of the sodium ion battery. And the addition of the carbon material with good conductive performance can just make up for the deficiency.
Disclosure of Invention
the invention takes tetravalent tin salt and thiourea as raw materials and is compounded with the carbon nano tube through a one-step hydrothermal process. The prepared material has a lamellar structure, the diameter is 1-3 mu m, the thickness is 1-20nm, the carbon nano tubes are independently and crossly loaded on the surface of a single sample, each lamellar sample is assembled into a flower shape, and finally the carbon nano tubes are loaded between the petals to form a loading network, thereby playing a good role of a conductive network. When the composite material is used as a negative electrode material of a sodium ion battery, the reversible capacity of the composite material is near 550mAh/g, and the SnS2/CNTs has good application prospect as the negative electrode material of the sodium ion battery.
the preparation scheme adopted by the invention is as follows:
(1) Adding carbon nano-tube into ultrapure water and carrying out ultrasonic treatment,
The specific measurement is as follows: adding 10-50mg of carbon nano tubes into 50mL of ultrapure water, and carrying out ultrasonic treatment for 3 h;
(2) adding SnCl4 & 5H2O solution into the dispersion system obtained in the step (1), adding thiourea after magnetic stirring, and carrying out magnetic stirring again,
Adding 7-10mL of SnCl 4.5H2O solution into the dispersion system in the step (1), magnetically stirring for 30min, then adding 2-7mmol of thiourea, magnetically stirring for 30min again,
Wherein, the SnCl4 & 5H2O solution takes hydrochloric acid as a solvent, the concentration of SnCl4 & 5H2O in the solution is 0.2mol/L, and the solute mass concentration of HCl is 36%;
(3) Carrying out hydrothermal reaction on the mixed system obtained in the step (2), cooling, filtering, washing and drying after the reaction to obtain the SnS2/CNTs composite nano material,
wherein the hydrothermal reaction temperature is 160-200 ℃, the reaction time is 300-900min,
After the hydrothermal treatment, the composite material is cooled to room temperature naturally, so that the composite material can change slowly in the cooling process, the size of the composite material is more uniform,
Drying at 60 deg.C for 6h by vacuum drying.
The invention also provides an application of the prepared SnS2/CNTs composite nano material in the aspect of preparing the cathode of the sodium-ion battery, which comprises the following specific steps:
according to the SnS2/CNTs composite nano material: super carbon: the sodium alginate is 60-80: 10-20: 10-20, adding the SnS2/CNTs composite nano material and super carbon into a sodium alginate aqueous solution with the mass concentration of 5%, fully mixing in a grinding state, preparing into uniform paste, uniformly coating the obtained paste on a copper foil as a substrate, drying, and drying in vacuum at 105 ℃ for 12h to obtain the sodium ion battery cathode,
in the traditional technology, a binder containing sodium ions is generally not used for a sodium battery material, because the existence of the sodium ions in the binder has negative influence on the performance of an electrode material; in the scheme of the invention, sodium alginate is used as the binder, and the sodium element contained in the binder has no influence on the performance of the sodium-ion battery electrode material.
Assembling the obtained negative electrode into a sodium ion battery: a battery case of model 2032 was used, the reference and reference electrodes were sodium sheets, the separator was Whatman GF/D, and the electrolyte was NaClO4 (at a concentration of 1 mol/L) dissolved in a mixture of PC-based electrolyte and fluoroethylene carbonate (FEC) (PC-based electrolyte to FEC volume ratio 100: 1).
The invention has the beneficial effects that:
According to the preparation method, the tetravalent tin salt and the thiourea are used as raw materials and are compounded with the carbon nano tube through a one-step simple hydrothermal process to prepare the SnS2/CNTs composite nano material, and the preparation method has the characteristics of mild reaction conditions, no pollution, simple process, high yield and the like;
the SnS2 material prepared by the method has a thin sheet structure, and the large specific surface area and the thin thickness of the SnS2 material provide a short de-intercalation channel for the movement of sodium ions in an active material, so that the material can have high reversible capacity;
the carbon nano tube is added, so that a complete conductive network can be formed on the surface of the SnS2 sheet material, a load is further formed between the sheets forming the flower shape, and an all-round supporting structure is formed for the whole flower shape SnS2, so that the SnS2 (namely petals) of the single sheet layer is supported, the connection and position relation between the sheets is consolidated, and the whole flower shape structure is more stable;
the defect of poor conductivity of a single SnS2 material is overcome, and compared with other carbon materials, the carbon nanotubes in the invention form a conductive network structure, so that the conductive effect of other carbon materials can be realized with a small addition amount, and the capacity loss caused by the addition of a large amount of carbon materials can be reduced as much as possible.
Drawings
FIG. 1 is an XRD image of the SnS2/CNTs composite nanomaterial obtained in example 1 of the present invention (obtained by testing with an X-ray diffractometer, model Rigaku D/max-2500/PC, Rigaku corporation, Japan), from which it can be seen that the main phase of the sample is hexagonal phase SnS2, the data of which is in accordance with the standard data (JCPDS 23-0677); while some of the peak positions identified by "#" in figure 1 illustrate the presence of carbon nanotubes.
FIG. 2 is a SEM (scanning electron microscope test using model SEM FEI INSPECT-F) of SnS2/CNTs composite nanomaterial obtained in example 1 of the present invention, from which it can be seen that carbon nanotubes are loaded on the surface of a single piece of Sn disulfide petals.
FIG. 3 is an all-dimensional SEM photograph (scanning electron microscope test using model SEM FEI INSPECT-F) of the SnS2/CNTs composite nanomaterial prepared in example 1, which shows that the prepared SnS2 is flower-shaped, and petals are connected to each other by loading of carbon nanotubes.
FIG. 4 is a comparison graph of constant current charging and discharging performance of SnS2/CNTs composite nano-materials prepared in inventive example 1 and comparative example 1 (measured on a blue light testing device with model number CT2001A, the charging and discharging current density is 20mA/g, the voltage range is 0.01-3V),
It can be seen that the cycling stability of the sample obtained in example 1 with internal support is significantly better than that of comparative example 1 without internal support.
Detailed Description
Example 1
(1) adding 50mg of carbon nanotubes into 50mL of ultrapure water, and carrying out ultrasonic treatment for 3 h;
(2) adding 7mL of SnCl4 & 5H2O solution (hydrochloric acid with the solute mass concentration of 36% is used as a solvent, the concentration of SnCl4 & 5H2O in the solution is 0.2mol/L), magnetically stirring for 30min, then adding 2.8mmol of thiourea, and magnetically stirring again for 30 min;
(3) carrying out 180 ℃ hydrothermal reaction on the mixed system obtained in the step (2) for 700min, naturally cooling to room temperature after reaction, carrying out suction filtration and water washing for 3 times, and putting the mixture into a vacuum drying oven for drying for 6h at 60 ℃ to obtain the SnS2/CNTs composite nano material;
preparing the SnS2/CNTs composite nano material into a negative electrode of a sodium ion battery:
According to the SnS2/CNTs composite nano material: super carbon: the sodium alginate is 80: 10: 10, adding the SnS2/CNTs composite nano material and the super carbon into a sodium alginate aqueous solution with the mass concentration of 5%, fully mixing in a grinding state, blending into uniform paste, uniformly coating the obtained paste on a copper foil serving as a substrate, drying, and performing vacuum drying at 105 ℃ for 12 hours to obtain a sodium ion battery cathode;
assembling the obtained negative electrode into a sodium ion battery: a battery case of model 2032 was used, the reference and reference electrodes were sodium sheets, the separator was Whatman GF/D, and the electrolyte was NaClO4 (at a concentration of 1 mol/L) dissolved in a mixture of PC-based electrolyte and fluoroethylene carbonate (FEC) (PC-based electrolyte to FEC volume ratio 100: 1).
The constant current charge and discharge test of the obtained battery is carried out on a blue test device (CT2001A), the charge and discharge current density is 20mA/g, the voltage range is 0.01-3V, and the detection result is shown in figure 4.
comparative example 1
(1) Measuring 50mL of ultrapure water;
(2) adding 7mL of SnCl4 & 5H2O solution (hydrochloric acid with the solute mass concentration of 36% is used as a solvent, the concentration of SnCl4 & 5H2O in the solution is 0.2mol/L) into the ultrapure water obtained in the step (1), magnetically stirring for 30min, then adding 2.8mmol of thiourea, and magnetically stirring again for 30 min;
(3) And (3) adding 50mg of carbon nanotubes into the mixed system obtained in the step (2), uniformly dispersing, carrying out hydrothermal reaction at 180 ℃ for 700min, naturally cooling to room temperature after reaction, carrying out suction filtration, washing for 3 times, and putting into a vacuum drying oven for drying at 60 ℃ for 6h to obtain the SnS2/CNTs composite nano material.
the procedures of preparing the SnS2/CNTs composite nano material obtained in the comparative example into the cathode of the sodium ion battery and then assembling the cathode into the sodium ion battery are the same as those of the example 1.
the constant current charge and discharge test of the battery obtained in the comparative example was performed on a blue test apparatus (CT2001A), the charge and discharge current density was 20mA/g, the voltage range was 0.01 to 3V, and the detection results are shown in fig. 4.
the data shown on the image of the attached figure 4 are analyzed, the first discharge specific capacities of the materials of the example 1 and the comparative example 1 can reach 721 and 719mAh/g respectively and are almost equal, but as the circulation is performed, the reversible capacity of the example 1 is obviously higher than that of the comparative example 1(568mAh/g VS 323mAh/g after 10 cycles), because compared with the comparative example 1, the carbon nano tube in the example 1 not only realizes large wrapping of the material, improves the conductivity of the single material, but also has special load on the surface of the single sheet, so that the material obtains more internal basic support, the structural stability of the material is more excellent, the irreversible volume change of the material when the material is used as a sodium ion battery cathode material is reduced, and more excellent cycle reversibility is obtained.
comparative example 2
Sodium alginate added when the negative electrode of the sodium-ion battery is prepared in the example 1 is replaced by carboxymethyl cellulose, and the preparation processes of all the other electrodes and batteries are the same as those in the example 1.
The constant current charge and discharge test of the battery obtained in this comparative example was performed on a blue test apparatus (CT2001A), the charge and discharge current density was 20mA/g, the voltage range was 0.01 to 3V, and the detection results almost coincided with the detection curve of example 1 in fig. 4, which indicates that: in the scheme of the invention, the sodium alginate used as the binder has no influence on the performance of the sodium-ion battery electrode material.
Claims (4)
1. a preparation method of SnS2/CNTs composite nano-material is characterized by comprising the following steps: the preparation method comprises the following steps of,
(1) Adding 10-50mg of carbon nano tubes into 50mL of ultrapure water, and carrying out ultrasonic treatment for 3 h;
(2) Adding 7-10mL of SnCl 4.5H2O solution into the dispersion system in the step (1), magnetically stirring for 30min, then adding 2-7mmol of thiourea, and magnetically stirring again for 30 min;
The SnCl4 & 5H2O solution takes hydrochloric acid as a solvent, and the concentration of SnCl4 & 5H2O in the solution is 0.2 mol/L;
(3) carrying out hydrothermal reaction on the mixed system obtained in the step (2), wherein the hydrothermal reaction temperature is 160-; the SnS2/CNTs composite nano material is structurally characterized in that a flower-shaped structure is assembled by SnS2 sheets with the diameter of 1-3 mu m and the thickness of 1-20nm loaded by carbon nano tubes, and the SnS2 sheets, the sheets and the sheets are connected and supported to form a stable network structure.
2. The method for preparing the SnS2/CNTs composite nano-material according to claim 1, characterized in that: in the step (3), drying is carried out for 6 hours at 60 ℃ in a vacuum drying mode.
3. The application of the SnS2/CNTs composite nano-material prepared by the method of any one of claims 1 to 2 as the negative electrode material of a sodium-ion battery.
4. the application of the SnS2/CNTs composite nano-material as the negative electrode material of the sodium-ion battery, which is claimed in claim 3, is characterized in that: the preparation method of the sodium ion battery cathode comprises the following steps of: super carbon: the sodium alginate is 60-80: 10-20: 10-20, adding the SnS2/CNTs composite nano material and super carbon into a sodium alginate aqueous solution with the mass concentration of 5%, fully mixing in a grinding state, preparing into uniform paste, uniformly coating the obtained paste on a copper foil serving as a substrate, drying, and drying in vacuum at 105 ℃ for 12 hours to obtain the sodium ion battery cathode.
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| CN107176590A (en) * | 2017-05-08 | 2017-09-19 | 太原理工大学 | Highly controllable ternary heterojunction structure material of constituent content and preparation method thereof |
| CN107394129A (en) * | 2017-06-20 | 2017-11-24 | 陕西科技大学 | A kind of preparation method of stannic disulfide carbon nano-tube combination electrode material |
| CN108878885A (en) * | 2018-07-03 | 2018-11-23 | 西南交通大学 | SnS2The preparation method of-CNTs composite material and preparation method and composite positive pole |
| CN109148857A (en) * | 2018-08-28 | 2019-01-04 | 中南大学 | A kind of preparation method of four vanadic sulfides of anode material of lithium-ion battery/carbon nanotube |
| CN110071279A (en) * | 2019-05-08 | 2019-07-30 | 陕西科技大学 | A kind of SnS2/ CNTs@rGO composite construction, preparation method and application |
| CN110165172A (en) * | 2019-05-17 | 2019-08-23 | 杭州求实新材料科技有限公司 | Fe for anode material of lithium-ion battery2+Support the preparation method of MXene |
| CN110148725A (en) * | 2019-05-21 | 2019-08-20 | 杭州求实新材料科技有限公司 | La for anode material of lithium-ion battery3+The preparation method of expanded support MXene |
| CN110844933B (en) * | 2019-11-29 | 2022-02-11 | 河北省科学院能源研究所 | Preparation method of stannous sulfide composite negative electrode material |
| CN115425204B (en) * | 2022-09-21 | 2024-03-29 | 陕西科技大学 | Biomass pine derived carbon PDC/SnS 2 @rGO material and preparation method and application thereof |
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